Hanna Instruments HI 84500 User Manual

Instruction Manual

HI 84500

FREE & TOTAL SULFUR DIOXIDE

MINITITRATOR

for wine analysis

www.hannainst.com

Dear Customer, Thank you for choosing a Hanna Instruments product. Please read this instruction manual carefully before using this instrument. This manual will

provide you with the necessary information for correct use of this instrument, as well as a precise idea of its versatility.

If you need additional technical information, do not hesitate to e-mail us at tech@hannainst.com or view our worldwide contact list at www.hannainst.com.

TABLE OF CONTENTS

PRELIMINARY EXAMINATION................................................................................................. 3

GENERAL DESCRIPTION ........................................................................................................ 3

SPECIFICATIONS ................................................................................................................... 5

PRINCIPLE OF OPERATION .................................................................................................... 6

FUNCTIONAL DESCRIPTION................................................................................................... 7

TITRATOR STARTUP ............................................................................................................. 9

SETUP MENU .................................................................................................................... 10

GUIDE TO DISPLAY CODES ................................................................................................... 13

ELECTRODE PREPARATION .................................................................................................. 16

DOSING PUMP INSTALLATION ............................................................................................. 17

DOSING PUMP PRIME PROCEDURE ..................................................................................... 17

ELECTRODE CHECK PROCEDURE .......................................................................................... 19

PUMP CALIBRATION PROCEDURE ........................................................................................ 19

FREE SO2 MEASUREMENT PROCEDURE................................................................................ 21

TOTAL SO2 MEASUREMENT PROCEDURE .............................................................................. 24

ORP MEASUREMENT .......................................................................................................... 28

PC INTERFACE AND DATA TRANSFER ................................................................................... 30

TROUBLESHOOTING GUIDE ................................................................................................ 31

ELECTRODE CONDITIONING AND MAINTENANCE .................................................................. 32

ACCESSORIES ..................................................................................................................... 34

WARRANTY........................................................................................................................ 35

All rights are reserved. Reproduction in whole or in part is prohibited without the written consent of the copyright owner, Hanna Instruments Inc., Woonsocket, Rhode Island, 02895, USA.

PRELIMINARY EXAMINATION

Please examine this product carefully. Make sure that the instrument is not damaged. If any damage occurred during shipment, please notify your Dealer.

Each HI 84500 minititrator is supplied complete with:

• HI 84500-70 Reagent Kit for SO2 determination

• HI 3148B ORP electrode

• HI 7082 Electrode Fill Solution (30 mL)

• Two 100 mL beakers

• Two 20 mL beakers

• Scissors

• Dosing Pump Valve

• 5 mL Syringe

• 1 mL Plastic Pipette

• Tube set (aspiration tube with titrant bottle cap and dispensing tube with tip)

• Stir bar

• Power Adapter

• Two sachets of cleaning solution for wine deposits

• Two sachets of cleaning solution for wine stains

• Instruction manual

Note:Save all packing material until you are sure that the instrument works correctly.

Any defective item must be returned in its original packing.

GENERAL DESCRIPTION

The HI 84500 is a low-cost, easy to use, microprocessor-based automatic titrator that benefits from Hanna’s years of experience as a manufacturer of analytical instrumentation.

The instrument incorporates a simple and reliable dosing pump which ensures high dosing reproducibility. Pump calibrations, performed with the provided Hanna reagents, assure the accuracy of the instrument.

The instrument comes with a preprogrammed method for Free and Total Sulfur Dioxide measurements in wine. The instrument uses a powerful algorithm which analyzes the shape of the electrode response in order to determine when the titration has reached completion.

The HI 84500 provides a simple user interface. By simply pressing the Start key in Titration mode, the instrument will automatically titrate the sample to the equivalence point and the results are immediately displayed in ppm. Another titration can be started immediately by pressing Restart.

Hp 0.3 1.3 2.3 3.3 4.3 5.3 6.3 7.3 8.3 9.3

OSeerF

41 81 22 82 53 44 55 96 78 901

A dedicated HELP key aids in setup, calibration, status and troubleshooting. Other features:

• ORP meter

• Stirrer speed control

• Graphic mode to display the titration data

• Data can be stored using the log feature and then exported to a USB stick or transferred to a PC using the USB connection

• Log on demand for up to 400 samples (200 for mV measurements; 200 for titration results)

• GLP feature, to view calibration data for the pump

SIGNIFICANCE OF USE

Wine makers add sulfur dioxide to wine in order to inhibit bacteria and wild yeast growth and to serve as an antioxidant to prevent browning. When SO2 is added to wine, a portion of it becomes immediately bound while a remaining portion is unbound SO2. The portion that is unbound is also called free; it is responsible for protecting the wine. The bound and unbound SO2 together are referred to as total SO2.

The relationship between the amount of SO2 added and the amount of free SO2 is complex. This relationship is governed by the total amount of SO2 in the wine. The exact relationship between free and bound will vary wine to wine. The amount of free SO2 depends on how much is added, how much was present before the addition and how much was immediately bound. Free SO2 exists in two forms. Bisulfite (HSO3¯) is the predominante form but is relatively ineffective. Molecular SO2 is the minor form and is responsible for protecting the wine. The amount of molecular SO2 available in wine is depended on the amount of free SO2 present and the pH. Typically 0.8 ppm of molecular SO2 provides adequate protection against bacteria growth and oxidation. In order to obtain this value for a wine sample that has a pH of 3.2 you would need 22 ppm of free SO2, if the pH was at 3.5 you would need double, 44 ppm.

Molecular SO2 can be detected by human senses at about 2.0 ppm. This level is needed for maximum protection of wine. Higher levels are needed for sweet and most notable, botrytised wine. The HI 84500

can be used to test for free and total SO2 in all wines, including red, which are difficult to test using traditional methods associated with a distinctive color change to determine the end point.

SPECIFICATIONS

Titrator Range Low Range: 1.0 to 40.0 ppm of SO

High Range: 30 to 400 ppm of SO

Resolution Low Range: 0.1 ppm

High Range: 1 ppm

Accuracy Low Range: 3% of reading or ±0.5 ppm @ 25 °C, whichever is greater

High Range: 3% of reading or ±1 ppm @ 25 °C, whichever is greater

Sample volume 50 mL Titration method Ripper method

Principle Equivalence point redox titration Pump speed 10 mL/min Stirring speed 700 rpm Log data Up to 200 samples

ORP meter ORP meter -2000.0 to 2000.0 mV

ORP Resolution 0.1 mV ORP Accuracy ± 1 mV Log data Up to 200 samples

ORP Electrode HI 3148B Environment 0 to 50 °C (32 to 122 °F); max 95% RH non-condensing Power supply 12 Vdc power adapter Dimensions 235 x 200 x 150 mm (9.2 x 7.9 x 5.9”) Weight 1.9 kg (67.0 oz.)

REQUIRED REAGENTS Code Description

HI 84500-50 Low Range Titrant HI 84500-51 High Range Titrant HI 84500-55 Calibration Standard HI 84500-60 Acid Reagent HI 84500-61 Alkaline Reagent (Total SO2) HI 84500-62 Stabilizer Packet

PRINCIPLE OF OPERATION

The HI 84500 determines the free and total sulfur dioxide concentration in wine using the Ripper method. Excess iodide added to the wine sample reacts with iodate introduced by the titrant to produce iodine.

+ 5I- + 6H

→ 3I

+ 3H2O

The iodine produced in the sample then reacts with sulfur dioxide in the wine according to the redox reaction below:

H2SO3 + I

→ H

2SO4

+ 2HI

The HI 84500 utilizes an ORP electrode to monitor the redox titration. The integrated algorithm detects when the reaction is complete (equivalence point). The volume of titrant required to reach the equivalence point, the titrant concentration and the sample size are used to calculate the sulfur dioxide concentration in the wine sample.

FUNCTIONAL DESCRIPTION

OVERHEAD VIEW

1) Titrant bottle

2) Liquid Crystal Display (LCD)

3) Keypad

4) Electrode holder

5) Dispensing tube

FRONT VIEW

REAR VIEW

6) ORP Electrode

7) Beaker

8) Dosing pump

9) Power switch

10) Power adapter

11) USB connector (PC interface)

12) USB connector (Storage interface)

13) BNC electrode connector

14) Titrant bottle

15) Syringe

16) Aspiration tube

17) Dosing Pump Valve

KEYPAD FUNCTION

ESC - used to leave the current screen and to return either to the previous screen or to the

main screen. In Setup menu, exits a parameter without changing the value.

/ - used to modify the parameter values, to scroll the information displayed while

viewing a help screen or to move between the options from the instrument’s Setup menu

CAL - used to access the Pump calibration HELP - used to access/exit the instrument’s contextual help LOG - used to save the current mV-ORP reading in ORP meter mode and the titration result MENU - used to enter Setup, Recall or GLP selection menu, while instrument is in ORP or

Titration mode

STIR - used to start/stop the stirrer

Note: The stirrer starts automatically during pump calibration and titration, it cannot

be stopped by pressing STIR key.

GUIDE TO INDICATORS

During the instrument’s operation information is displayed on the LCD. Displayed icons:

Unstable reading.Stirrer on. Pump running.

Stirrer is not working properly.

1) Current time and instrument mode information (ORP meter or Titrator)

2) Instrument status

3) Virtual option keys

4) Stirrer and reading status

5) Main reading information

Parameter can be modified.

DOSING PUMP

The dosing pump is based on a valve that automatically moves the titrant between the titrant bottle and syringe when filling the syringe and between the syringe and sample when dispensing. A replaceable 5 mL plastic syringe is used to limit the amount of titrant used per test to ensure the highest possible accuracy. Before a set of titrations, it is necessary to prime the dosing system.

Note: Once titrations have been completed, the dosing system should be cleaned with deionized

water using the prime feature.

TITRATOR STARTUP

This is a general outline of the steps required to perform a titration. The following topics are expanded upon in each section that follows.

• Place the instrument on a flat table. Do not place the instrument in direct sun light.

• Connect the power adapter to the instrument.

• Turn the instrument ON using the power switch from the rear panel of the instrument.

• Set up the instrument. See the “Setup Menu” section for details.

• Connect the ORP sensor to the instrument.

• Connect the tubes and the valve. See the “Dosing Pump Installation” section for the procedure.

• Remove the titrant bottle cap and replace it with the bottle cap with tubes. Place the titrant bottle in the appropriate place on the titrator top.

Note: Different titrants are required based on the concentration. See “Pump Calibration Procedure”

for details.

• Prime the syringe. To assure high accuracy, verify there are no air bubbles in the syringe or tubing.

• Calibrate the pump.

Note: Different volumes of standard are required based on the concentration. See “Pump

Calibration Procedure” for details.

• Prepare the sample.

• Run a titration and log sample results.

SETUP MENU

The titrator’s setup menu may be accessed from the main screen (meter or titrator mode) by pressing the MENU key, then Setup.

A list of setup parameters will be displayed with currently configured setting. While in the setup menu it is possible to modify the instrument’s operation parameters. The

ARROW keys permit the user to scroll the setup parameters. Press HELP to view the contextual help. Press ESC to return to the main screen.

Range Setup

Use Low measurement range for 1.0 - 40.0 ppm. Use High measurement range for 30 - 400 ppm.

Use the appropriate titrant for each range.

To ensure a high accuracy, it is recommended to recalibrate the pump after the valve, titrant or electrode has been changed.

Time

Press the Modify key to change the time and time format.

Date

Press Format to switch between 12 hour (am/pm) and 24 hour mode. Press to highlight the value to be modified. Use the ARROW keys to change the value. Press Accept to confirm the new value or ESC to return to the setup.

Press the Modify key to change the date and date format.

Key Beep

Error Beep

Decimal Separator

Press Format to cycle between the available date formats. Press to highlight the value to be modified. Use the ARROW keys to change the value. Press Accept to confirm the new value or ESC to return to the setup.

Select Enable to activate or Disable to deactivate the Key Beep function.

If enabled, a short beep will be heard every time a key is pressed.

Select Enable to activate or Disable to deactivate the Error Beep function.

If enabled, a beep will be heard when an error condition occurs.

This option allows the user to select the symbol used for a decimal separator.

LCD Contrast

This option is used to set the display’s contrast. Press Modify to change the display’s contrast. The default value is 8.

Use the ARROW keys or / to increase/ decrease the value. Press Accept to confirm the value or ESC to return to the setup menu.

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